CN102806018B - Method for lower-temperature sintering to prepare acid and alkali-resistant titanium dioxide ceramic ultrafiltration membrane - Google Patents
Method for lower-temperature sintering to prepare acid and alkali-resistant titanium dioxide ceramic ultrafiltration membrane Download PDFInfo
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- CN102806018B CN102806018B CN201210242295.4A CN201210242295A CN102806018B CN 102806018 B CN102806018 B CN 102806018B CN 201210242295 A CN201210242295 A CN 201210242295A CN 102806018 B CN102806018 B CN 102806018B
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Abstract
The invention relates to a method for lower-temperature sintering to prepare an acid and alkali-resistant titanium dioxide ceramic ultrafiltration membrane. The method takes titanyl sulfate, ammonium oxalate or oxalic acid as a raw material, is combined with a technology of preparing small nanometer materials through a sol-gel method and a solid particle sintering technology, so the technology for preparing the acid and alkali-resistant titanium dioxide ceramic ultrafiltration membrane under the low-temperature sintering condition is obtained. The layer pore size distribution scope of the ceramic ultrafiltration membrane which is produced by the method is between 10-30nm, and the water flux under the operation condition of 0.1MPa is 400-600L/m<3>h; and the prepared ceramic ultrafiltration membrane has very good acid resistance and alkali resistance and brighter application prospect. The method uses inorganic titanium salt with lower price as the raw material for synthetizing titanium dioxide, so the preparation cost of the ceramic membrane is lowered; and moreover, compared with a solid particle high-temperature sintering technology of the existing ceramic membrane industrial production, the method adopts a lower-temperature sintering technology, so the energy consumption is reduced, and the produced product has higher cost performance.
Description
Technical field
The present invention relates to a kind of preparation method of Ceramic excessive filtration rete, be specifically related to a kind of method that low-temperature sintering is prepared acid and alkali-resistance titanium dioxide ceramic ultrafiltration rete.
Background technology
Ceramic membrane compare organic film have high temperature resistant, chemical stability good, mechanical strength is high, resistance to microorganism, long service life, cyclic utilization rate is high, aperture is controlled and pollute the advantages such as little, can meet the harsher occasions of condition such as high soda acid, high temperature, developed rapidly in recent years, be widely used in the various fields such as chemical industry, food, environmental protection, bioengineering.According to the difference of separation principle and fenestra size, ceramic membrane can be divided into micro-filtration, ultrafiltration, nanofiltration and counter-infiltration etc.Milipore filter aperture generally between 2 ~ 50nm, has good rejection effect for large molecule and little molecule or ultra-fine grain, can be applicable to purify, concentrated, the tiny colloid thing of classification or large molecule.Ceramic super-filtering film is not only with a wide range of applications aspect fluid separation applications, and is the basis of gas separation membrane and catalytic membrane.Along with the expansion of ceramic super-filtering film application to fields such as gas separation and film catalysis, the stable of physics and chemistry performance to ceramic super-filtering film had higher requirement, and the ceramic super-filtering film of therefore preparing physics and chemistry stable performance becomes the focus in ceramic membrane research field.Selection and the preparation method of the control of the physical and chemical performance of ceramic film and ceramic film material have close relationship.Conventional ceramic membrane materials has Al
2o
3, ZrO
2, SiO
2and TiO
2deng.But the preparation cost of this based ceramic film is compared, organic film is higher, makes its application be subject to certain restriction.Conventionally the preparation method of ceramic membrane is divided into two steps, the one, the preparation of supporter, the 2nd, the preparation of separating layer, first prepare the supporter with larger aperture, by methods such as solid particles sintering process, cement-dipping method, anodizing, spray heating decomposition, chemical vapour deposition techniques, on supporter, prepare separated rete again, form the ceramic membrane with two-layer or two-layer above dissymmetrical structure.In separation process, its main centrifugation be separated rete.The preparation of general supporter and separating layer is separately carried out, and sintering process cost in whole ceramic membrane preparation process is maximum, and therefore reducing sintering temperature has obvious effect to reducing the preparation cost of ceramic membrane.But the reduction of sintering temperature also makes the physics and chemistry performance of ceramic membrane simultaneously, and performances such as mechanical strength, acid and alkali-resistance, has obvious decline.
Summary of the invention
The present invention be take titanyl sulfate, ammonium oxalate or oxalic acid as raw material, prepares technology and the solid particles sintering technology of small size nano material in conjunction with sol-gel process, obtains the technology of preparing acid and alkali-resistance titanium dioxide ceramic milipore filter under low-temperature sintering condition.
Technical scheme of the present invention is as follows:
Low-temperature sintering is prepared a method for acid and alkali-resistance titanium dioxide ceramic milipore filter, comprises following steps:
(1) titanyl sulfate solution of preparation, at room temperature stirring and dissolving, removes insoluble matter with Filter paper filtering solution; Dispersant is directly added in the titanyl sulfate solution after filtration and mixed, keeping under the condition of reaction temperature, rate of addition and mixing speed, ammonium oxalate or oxalic acid solution are added drop-wise in titanyl sulfate solution, after stirring reaction is complete, with frozen water is cooling, make Precipitation in solution, filtering precipitate is also repeatedly recrystallized after removing foreign ion and is configured to titanium oxalate solution sediment with oxalic acid or ammonium oxalate solution; With ammoniacal liquor, the pH value of solution is adjusted to 6-9, heating stirs;
(2) by the titanium oxalate solution evaporate to dryness preparing, the titanium oxalate solid obtaining is calcined to the nano TiO 2 powder preparing;
(3) after the nano TiO 2 powder preparing is dry grinded by ceramic mortar, add dispersant and water carry out wet-milling and are configured to nano titanium oxide dispersion;
(4) in nano titanium oxide dispersion, add coalescents, drying control agent, defoamer to make coating liquid;
(5) this coating liquid is applied on porous ceramic film support, through super-dry, sintering, obtains titanium dioxide ceramic milipore filter rete.
Described step is converted into titanium dioxide equivalent by titanyl sulfate in (1), and in titanyl sulfate solution, titanium dioxide mass content is 0.5%-5%; Dispersant is commercial dispersant, its model be in disper740w, disper750w, disper752w any one or multiple; In mixed solution, the mass content of dispersant is 0.5%-5%, and the mol ratio of ammonium oxalate or oxalic acid and titanyl sulfate is that 1:1 is to 1:2; Reaction temperature is 25 ℃-60 ℃.After recrystallization, heating whipping temp is 60 ℃-100 ℃
After recrystallization removal of impurities, the titanium oxalate solution concentration of preparation is: titanium dioxide mass content is 0.5-5%.
In described step (2), the calcining heat of titanium dioxide is 400 ℃-700 ℃.
The Ginding process of the nano TiO 2 powder preparing in described step (3) is for after first dry grinding by ceramic mortar, then adds dispersant and water to carry out wet-milling.Dispersant is commercial dispersant, its model be in disper740w, disper750w, disper752w any one or multiple; Dispersant, water and titanium dioxide mass fraction ratio are respectively 10%-200% and 50%-100%.
In described step (4), in nano titanium oxide dispersion, titanium dioxide mass fraction content is 1%-5%.
In described step (4), coalescents is polyvinyl alcohol, and coalescents accounts for the 5%-500% of titanium dioxide quality.
In described step (4), drying control agent is one or several in ethylene glycol, butanediol, glycerine, and in drying control agent quality and coating liquid, the ratio of water quality is 5%-100%.
In described step (4), defoamer is silicone defoaming agent, and its quality accounts for the 0.01%-0.1% of coating liquid quality.
Drying condition in described step (5) is room temperature to 100 ℃, and be greater than 2 hours drying time.
Sintering condition in described step (5) is a certain temperature in the temperature programming to 400 of 0.5～4 ℃/min ℃～900 ℃, and constant temperature is cooling naturally after 2～5 hours.
The present invention be take titanyl sulfate, ammonium oxalate or oxalic acid as raw material, prepares technology and the solid particles sintering technology of small size nano material in conjunction with sol-gel process, obtains the technology of preparing acid and alkali-resistance titanium dioxide ceramic milipore filter under low-temperature sintering condition.The rete pore size distribution range of the ceramic super-filtering film that the method is produced is 10-30nm, and under 0.1MPa operating condition, water flux is 400-600L/m
3h; The ceramic super-filtering film preparing is in the sodium hydroxide solution of 20% sulfuric acid and 5%, and 75 ℃ of little immersions of condition 4 days, its rete aperture and mechanical strength did not change, and have good anti acid alkali performance energy.It is the synthetic raw material of titanium dioxide that the present invention has used the inorganic titanium salt that price is comparatively cheap, has reduced the preparation cost of ceramic membrane; Meanwhile, the solid particles high temperature sintering technology of comparing in current ceramic membrane industrial production, the present invention has adopted low-temperature sintering technology, has reduced energy consumption, makes the product of producing have higher cost performance.
Accompanying drawing explanation
Accompanying drawing is the electronic scanner microscope figure after the titanium dioxide ceramic milipore filter for preparing by low-temperature sintering method of the embodiment of the present invention 1 and its soak 4 days through 20% sulfuric acid under 75 ℃ of conditions.Fig. 1 and 3 is the multiplication factor Electronic Speculum figure that is 500, Fig. 2 and 4 for multiplication factor be the Electronic Speculum figure of 100,000 times.The titanium dioxide ceramic ultrafiltration even film layer that this invention prepares is as can be seen from Figure 1 without cracking; The Ceramic excessive filtration rete pore-size distribution that this invention prepares is as can be seen from Figure 2 at 10-30nm, and porosity is higher; From Fig. 2 and 4, can find out that titanium dioxide ceramic milipore filter that this invention prepares its rete and aperture after 20% sulfuric acid soaks 4 days under 75 ℃ of conditions do not change.
The data unit of providing: Chemistry and Chemical Engineering College of Xiamen University
Instrument model: HITACHI S-4800 ESEM
The specific embodiment
Embodiment 1
Titanyl sulfate is converted into titanium dioxide equivalent, and the titanyl sulfate solution that configuration titanium dioxide mass content is 2.5%, at room temperature stirs dissolving in 4 hours, with 4 layers of Medium speed filter paper solids removed by filtration impurity, the dispersant disper740w that takes certain mass adds in titanyl sulfate solution, be mixed with dispersant mass fraction and be 1% solution, and mix, 25 ℃ of reaction temperatures, under fixing rate of addition and the condition of mixing speed, by the mol ratio with titanyl sulfate, be that 1:1.2 ammonium oxalate or oxalic acid solution are added drop-wise in titanyl sulfate solution, after stirring reaction 1 hour, with ice-water bath is cooling, make Precipitation in solution, filtering precipitate is also repeatedly recrystallized and removes foreign ion and obtain the less titanium oxalate of impurity content and precipitate sediment with 1% oxalic acid or ammonium oxalate solution, titanium oxalate is scaled to titanium dioxide equivalent, and it is 2.5% titanium oxalate solution that the titanium oxalate precipitation obtaining is configured to titanium dioxide mass content, with ammoniacal liquor, the pH of solution is adjusted to 7, under 80 ℃ of conditions, continues stirring reaction 1 hour, by the titanium oxalate colloidal sol evaporate to dryness preparing, the titanium oxalate solid obtaining is calcined under 500 ℃ of conditions, after the nano TiO 2 powder preparing is dry grinded by ceramic mortar, to add with titanium dioxide mass fraction ratio be that 20% dispersant disper740w and 50% water carries out wet-milling and be configured to concentration is 2.5% nano titanium oxide dispersion, in the titanium oxide dispersion that is 2.5% in concentration, add the polyvinyl alcohol that accounts for titanium dioxide quality 50% as coalescents, add with coating liquid in the ratio of the water quality glycerine that is 80% as drying control agent, add the silicone defoaming agent that accounts for coating liquid quality 0.01% to make coating liquid, this coating liquid is applied on porous ceramic film support, under 80 ℃ of conditions through 5 hours dry, through the temperature programming to 700 ℃ of 4 ℃/min, constant temperature naturally was lowered the temperature and is obtained titanium dioxide ceramic milipore filter rete after 3 hour.
Embodiment 2
Titanyl sulfate is converted into titanium dioxide equivalent, and the titanyl sulfate solution that configuration titanium dioxide mass content is 5%, at room temperature stirs dissolving in 4 hours, with 4 layers of Medium speed filter paper solids removed by filtration impurity, the dispersant disper750w that takes certain mass adds that in titanyl sulfate solution, to be mixed with dispersant mass fraction be that 5% solution mixes, 50 ℃ of reaction temperatures, under fixing rate of addition and the condition of mixing speed, by the mol ratio with titanyl sulfate, be that 1:1.5 ammonium oxalate or oxalic acid solution are added drop-wise in titanyl sulfate solution, after stirring reaction 1 hour, with ice-water bath is cooling, make Precipitation in solution, filtering precipitate is also repeatedly recrystallized and removes foreign ion and obtain the less titanium oxalate of impurity content and precipitate sediment with 1% oxalic acid or ammonium oxalate solution, titanium oxalate is scaled to titanium dioxide equivalent, and it is 5% titanium oxalate solution that the titanium oxalate precipitation obtaining is configured to titanium dioxide mass content, with ammoniacal liquor, the pH of solution is adjusted to 8, under 60 ℃ of conditions, continues stirring reaction 2 hours, by the titanium oxalate colloidal sol evaporate to dryness preparing, the titanium oxalate solid obtaining is calcined under 400 ℃ of conditions, after the nano TiO 2 powder preparing is dry grinded by ceramic mortar, to add with titanium dioxide mass fraction ratio be that 200% dispersant disper752w and 100% water carries out wet-milling and be configured to concentration is 1% nano titanium oxide dispersion, in the titanium oxide dispersion that is 1% in concentration, add the polyvinyl alcohol that accounts for titanium dioxide quality 5% as coalescents, add with coating liquid in the ratio of the water quality ethylene glycol that is 100% as drying control agent, add the silicone defoaming agent that accounts for coating liquid quality 0.1% to make coating liquid, this coating liquid is applied on porous ceramic film support, and dry through 5 hours under 50 ℃ of conditions, through the temperature programming to 500 ℃ of 2 ℃/min, constant temperature was naturally lowered the temperature and is obtained titanium dioxide ceramic milipore filter rete after 4 hour.
Embodiment 3
Titanyl sulfate is converted into titanium dioxide equivalent, and the titanyl sulfate solution that configuration titanium dioxide mass content is 0.5%, at room temperature stirs dissolving in 4 hours, with 4 layers of Medium speed filter paper solids removed by filtration impurity, the dispersant disper752w that takes certain mass adds that in titanyl sulfate solution, to be mixed with dispersant mass fraction be that 0.5% solution mixes, 60 ℃ of reaction temperatures, under fixing rate of addition and the condition of mixing speed, by the mol ratio with titanyl sulfate, be that 1:1 ammonium oxalate or oxalic acid solution are added drop-wise in titanyl sulfate solution, after stirring reaction 1 hour, with ice-water bath is cooling, make Precipitation in solution, filtering precipitate is also repeatedly recrystallized and removes foreign ion and obtain the less titanium oxalate of impurity content and precipitate sediment with 1% oxalic acid or ammonium oxalate solution, titanium oxalate is scaled to titanium dioxide equivalent, and it is 0.5% titanium oxalate solution that the titanium oxalate precipitation obtaining is configured to titanium dioxide mass content, with ammoniacal liquor, the pH of solution is adjusted to 6, under 100 ℃ of conditions, continues stirring reaction 1 hour, by the titanium oxalate colloidal sol evaporate to dryness preparing, the titanium oxalate solid obtaining is calcined under 600 ℃ of conditions, after the nano TiO 2 powder preparing is dry grinded by ceramic mortar, to add with titanium dioxide mass fraction ratio be that 10% dispersant disper750w and 80% water carries out wet-milling and be configured to concentration is 3% nano titanium oxide dispersion, in the titanium oxide dispersion that is 3% in concentration, add the polyvinyl alcohol that accounts for titanium dioxide quality 500% as coalescents, add with coating liquid in the ratio of the water quality butanediol that is 5% as drying control agent, add the silicone defoaming agent that accounts for coating liquid quality 0.1% to make coating liquid, this coating liquid is applied on porous ceramic film support, under 100 ℃ of conditions through 2 hours dry, through the temperature programming to 600 ℃ of 0.5 ℃/min, constant temperature naturally was lowered the temperature and is obtained titanium dioxide ceramic milipore filter rete after 2 hour.
Embodiment 4
Titanyl sulfate is converted into titanium dioxide equivalent, and the titanyl sulfate solution that configuration titanium dioxide mass content is 2%, at room temperature stirs dissolving in 4 hours, with 4 layers of Medium speed filter paper solids removed by filtration impurity, the dispersant disper740w that takes certain mass adds that in titanyl sulfate solution, to be mixed with dispersant mass fraction be that 3% solution mixes, 40 ℃ of reaction temperatures, under fixing rate of addition and the condition of mixing speed, by the mol ratio with titanyl sulfate, be that 1:2 ammonium oxalate or oxalic acid solution are added drop-wise in titanyl sulfate solution, after stirring reaction 1 hour, with ice-water bath is cooling, make Precipitation in solution, filtering precipitate is also repeatedly recrystallized and removes foreign ion and obtain the less titanium oxalate of impurity content and precipitate sediment with 1% oxalic acid or ammonium oxalate solution, titanium oxalate is scaled to titanium dioxide equivalent, and it is 2% titanium oxalate solution that the titanium oxalate precipitation obtaining is configured to titanium dioxide mass content, with ammoniacal liquor, the pH of solution is adjusted to 9, under 70 ℃ of conditions, continues stirring reaction 2 hours, by the titanium oxalate colloidal sol evaporate to dryness preparing, the titanium oxalate solid obtaining is calcined under 700 ℃ of conditions, after the nano TiO 2 powder preparing is dry grinded by ceramic mortar, to add with titanium dioxide mass fraction ratio be that 100% mixed dispersant (disper740w:disper752w=1:3) and 50% water carries out wet-milling and be configured to concentration is 5% nano titanium oxide dispersion, in the titanium oxide dispersion that is 5% in concentration, add the polyvinyl alcohol that accounts for titanium dioxide quality 300% as coalescents, add with coating liquid in the ratio of the water quality glycerine that is 50% as drying control agent, add the silicone defoaming agent that accounts for coating liquid quality 0.05% to make coating liquid, this coating liquid is applied on porous ceramic film support, and dry through 2 days at ambient temperature, through the temperature programming to 400 ℃ of 1 ℃/min, constant temperature was naturally lowered the temperature and is obtained titanium dioxide ceramic milipore filter rete after 5 hour.
Embodiment 5
Titanyl sulfate is converted into titanium dioxide equivalent, and the titanyl sulfate solution that configuration titanium dioxide mass content is 4%, at room temperature stirs dissolving in 4 hours, with 4 layers of Medium speed filter paper solids removed by filtration impurity, the mixed dispersant (disper740w:disper750w=1:2) that takes certain mass adds that in titanyl sulfate solution, to be mixed with dispersant mass fraction be that 2% solution mixes, 25 ℃ of reaction temperatures, under fixing rate of addition and the condition of mixing speed, by the mol ratio with titanyl sulfate, be that 1:1.8 ammonium oxalate or oxalic acid solution are added drop-wise in titanyl sulfate solution, after stirring reaction 1 hour, with ice-water bath is cooling, make Precipitation in solution, filtering precipitate is also repeatedly recrystallized and removes foreign ion and obtain the less titanium oxalate of impurity content and precipitate sediment with 1% oxalic acid or ammonium oxalate solution, titanium oxalate is scaled to titanium dioxide equivalent, and it is 4% titanium oxalate solution that the titanium oxalate precipitation obtaining is configured to titanium dioxide mass content, with ammoniacal liquor, the pH of solution is adjusted to 8, under 100 ℃ of conditions, continues stirring reaction 1 hour, by the titanium oxalate colloidal sol evaporate to dryness preparing, the titanium oxalate solid obtaining is calcined under 500 ℃ of conditions, after the nano TiO 2 powder preparing is dry grinded by ceramic mortar, adding with titanium dioxide mass fraction ratio is 200% mixed dispersant (disper740w:disper752w=1: 1) and 60% water carries out wet-milling and is configured to concentration is 2% nano titanium oxide dispersion, in the titanium oxide dispersion that is 2% in concentration, add the polyvinyl alcohol that accounts for titanium dioxide quality 200% as coalescents, add with coating liquid in the ratio of the water quality ethylene glycol that is 20% as drying control agent, add the silicone defoaming agent that accounts for coating liquid quality 0.08% to make coating liquid, this coating liquid is applied on porous ceramic film support, under 40 ℃ of conditions through 2 days dry, through the temperature programming to 900 ℃ of 3 ℃/min, constant temperature naturally was lowered the temperature and is obtained titanium dioxide ceramic milipore filter rete after 2 hour.
The above, be only preferred embodiment of the present invention, therefore can not limit according to this scope of the invention process, the equivalence done according to the scope of the claims of the present invention and description changes and modifies, and all should still belong in the scope that the present invention contains.
Claims (9)
1. low-temperature sintering is prepared a method for acid and alkali-resistance titanium dioxide ceramic milipore filter, it is characterized in that comprising following steps:
(1) preparation titanyl sulfate solution, at room temperature stirring and dissolving, removes insoluble matter with Filter paper filtering solution; Dispersant is directly added in the titanyl sulfate solution after filtration and mixed, keeping under the condition of reaction temperature, rate of addition and mixing speed, ammonium oxalate or oxalic acid solution are added drop-wise in titanyl sulfate solution, after stirring reaction is complete, with frozen water is cooling, make Precipitation in solution, filtering precipitate is also repeatedly recrystallized after removing foreign ion and is configured to titanium oxalate solution sediment with oxalic acid or ammonium oxalate solution; With ammoniacal liquor, the pH value of solution is adjusted to 6-9, heating stirs;
(2) by the titanium oxalate solution evaporate to dryness preparing, the titanium oxalate solid obtaining is calcined to the nano TiO 2 powder preparing;
(3) after the nano TiO 2 powder preparing is dry grinded by ceramic mortar, add dispersant and water carry out wet-milling and are configured to nano titanium oxide dispersion;
(4) in nano titanium oxide dispersion, add coalescents, drying control agent, defoamer to make coating liquid;
(5) this coating liquid is applied on porous ceramic film support, through super-dry, sintering, obtains titanium dioxide ceramic milipore filter rete;
Wherein, described step is converted into titanium dioxide equivalent by titanyl sulfate in (1), and in titanyl sulfate solution, titanium dioxide mass content is 0.5%-5%; In mixed solution, the mass content of dispersant is 0.5%-5%, and the mol ratio of ammonium oxalate or oxalic acid and titanyl sulfate is that 1:1 is to 1:2; Reaction temperature is 25 ℃-60 ℃; After recrystallization, heating whipping temp is 60 ℃-100 ℃.
2. a kind of low-temperature sintering as claimed in claim 1 is prepared the method for acid and alkali-resistance titanium dioxide ceramic milipore filter, it is characterized in that: in described step (2), the calcining heat of titanium dioxide is 400 ℃-700 ℃.
3. a kind of low-temperature sintering as claimed in claim 1 is prepared the method for acid and alkali-resistance titanium dioxide ceramic milipore filter, it is characterized in that: the Ginding process of the nano TiO 2 powder preparing in described step (3) is for after first dry grinding by ceramic mortar, then add and disperse and water carries out wet-milling; Dispersant, water and titanium dioxide mass fraction ratio are respectively 10%-200% and 50%-100%.
4. a kind of low-temperature sintering as claimed in claim 1 is prepared the method for acid and alkali-resistance titanium dioxide ceramic milipore filter, it is characterized in that: in described step (4), in nano titanium oxide dispersion, titanium dioxide mass fraction content is 1%-5%.
5. a kind of low-temperature sintering as claimed in claim 1 is prepared the method for acid and alkali-resistance titanium dioxide ceramic milipore filter, it is characterized in that: in described step (4), coalescents is polyvinyl alcohol, and coalescents accounts for the 5%-500% of titanium dioxide quality.
6. a kind of low-temperature sintering as claimed in claim 1 is prepared the method for acid and alkali-resistance titanium dioxide ceramic milipore filter, it is characterized in that: in described step (4), drying control agent is one or several in ethylene glycol, butanediol, glycerine, and in drying control agent quality and coating liquid, the ratio of water quality is 5%-100%.
7. a kind of low-temperature sintering as claimed in claim 1 is prepared the method for acid and alkali-resistance titanium dioxide ceramic milipore filter, it is characterized in that: in described step (4), defoamer is silicone defoaming agent, and its quality accounts for the 0.01%-0.1% of coating liquid quality.
8. a kind of low-temperature sintering as claimed in claim 1 is prepared the method for acid and alkali-resistance titanium dioxide ceramic milipore filter, it is characterized in that: the drying condition in described step (5) is room temperature to 100 ℃, and be greater than 2 hours drying time.
9. a kind of low-temperature sintering as claimed in claim 1 is prepared the method for acid and alkali-resistance titanium dioxide ceramic milipore filter, it is characterized in that: the sintering condition in described step (5) is for through the temperature programming to 400 of 0.5～4 ℃/min ℃～900 ℃, and constant temperature is lowered the temperature after 2～5 hours naturally.
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| CN103041795A (en) * | 2012-12-27 | 2013-04-17 | 广西大学 | Preparation method of titanium dioxide photocatalyst |
| CN103752186B (en) * | 2014-01-26 | 2015-09-16 | 成都新柯力化工科技有限公司 | A kind of preparation method of ceramic super-filtering film |
| CN104446400B (en) * | 2014-12-23 | 2017-01-04 | 苏州宽温电子科技有限公司 | A kind of composite ceramic material of acid and alkali-resistance and preparation method thereof |
| CN105903351B (en) * | 2016-06-14 | 2018-12-25 | 浙江瑞奕环保股份有限公司 | A kind of ceramic super-filtering film and preparation method thereof with self-cleaning function |
| CN106178981B (en) * | 2016-08-12 | 2018-10-26 | 三达膜科技（厦门）有限公司 | A kind of method of low temperature preparation titanium oxide ceramics ultrafiltration membrane |
| DE102018123437A1 (en) * | 2018-09-24 | 2020-03-26 | Endress+Hauser Conducta Gmbh+Co. Kg | Diaphragm and half-cell with diaphragm for an electrochemical sensor and manufacturing process thereof |
| CN112759370A (en) * | 2019-10-18 | 2021-05-07 | 三达膜科技（厦门）有限公司 | Preparation method of high-strength ceramic filtering membrane |
| CN112939580B (en) * | 2021-01-29 | 2022-07-01 | 广西碧清源环保投资有限公司 | Preparation method of ceramic filtering membrane |
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